CN108975794A - Clay/sodium alginate composite aerogel fire proofing and preparation method thereof - Google Patents
Clay/sodium alginate composite aerogel fire proofing and preparation method thereof Download PDFInfo
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- CN108975794A CN108975794A CN201811054063.XA CN201811054063A CN108975794A CN 108975794 A CN108975794 A CN 108975794A CN 201811054063 A CN201811054063 A CN 201811054063A CN 108975794 A CN108975794 A CN 108975794A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/001—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing unburned clay
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/28—Fire resistance, i.e. materials resistant to accidental fires or high temperatures
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/20—Mortars, concrete or artificial stone characterised by specific physical values for the density
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
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Abstract
The present invention relates to clay field of deep, a kind of clay/sodium alginate composite aerogel fire proofing and preparation method thereof is disclosed, which is grouped as by the group of following mass ratio: clay: calcium carbonate: sodium alginate: gluconolactone=100:1 ~ 5:5:1.75.Using clay as raw material, improve the mechanical performance of aeroge using sodium alginate, using Isopropanol Water Solvent Mixtures, gained hydrogel is chilled, isopropanol solvent is replaced and constant pressure and dry obtains.Composite aerogel aperture is mainly distributed on 5nm, and for porosity up to 98.8%, apparent density is 0.03 ~ 0.06gcm‑3, thermal coefficient is 0.020 ~ 0.032W/ (mk).This heat-isolating flame retardant material has good application prospect in addition to excellent fire-retardancy, good mechanical performance meets the requirement of ecological, environmental protective, and process cycle is short, and solvent consumption is few, and production cost is low, in the flame resistant heat insulation material field of building.
Description
Technical field
The present invention relates to clay field of deep, in particular to a kind of clay/sodium alginate composite aerogel anti-flaming thermal-insulation
Material and its preparation process.
Background technique
" super " thermal insulation material of aeroge as rising in recent years, thermal coefficient are far below common insulating foam.Clay/
Macromolecule composite aerogel is having inorganic and organic aerogel excellent properties as newborn third generation material, such as comes
Source is abundant, degradable and biocompatibility, has huge potentiality in following heat-barrier material.
The research for preparing anti-flaming thermal-insulation aerogel material using clay is raw material, in recent years by the extensive of researchers
Concern.Wang et al. reports 20-40wt% furfuryl alcohol and mixes with 10wt% nano inorganic mineral bentonite slurry 1:1, passes through freezing
It is 0.117g-0.179g/cm that density, which is prepared, in dry technology3Aerogel composite.The inflammability of the composite aerogel is low,
Bearing the unobvious burning of gas flame is more than nearly 20 seconds (Wang T, Sun H, Long J, et al. ACS
Sustainable Chemistry & Engineering2016, 4 (5), 2601-2605.).Zhao et al., which is reported, to be adopted
With 5wt% bentonite, it is 0.118g/ that density, which is prepared, by Freeze Drying Technique in 5wt%PVA and 2wt% pig gelatin or isinglass
cm3Composite aerogel.The limit oxygen index (LOI) of gained aeroge can reach 28.5%(Wang Y T, Zhao H Bo
, Degracia K et al. Acs Applied Materials & Interfaces, 2017, 9, 42258-
42265).
Relative to traditional Supercritical Drying Technology, Freeze Drying Technique environmentally friendly at present is to prepare clay/height
The most common drying means of Molecularly Imprinted Polymer composite aerogel.But there is still a need for relatively low temperature, certain pressure for freeze-drying
The deficiencies of strong range and higher equipment investment, limits clay/high molecular polymer composite aerogel in building anti-flaming thermal-insulation
Application.For constant pressure and dry technology using conventional atmospheric pressure device, equipment investment is low, and operation is seen, and does not need condition of high voltage and spy
Fixed reactor, it is easy to accomplish large-scale production, particularly suitable for producing the dedicated aerogel material of building heat preservation.But it is existing
Deficiency is, aeroge is easily collapsed due to the effect aeroge of capillary pressure in drying process.
Wet gel constant pressure and dry causes aeroge to collapse in order to prevent, at present frequently with repeatedly to wet gel solvent displacement,
Surface is modified to be increased the technological means such as supporter and reduces aeroge and collapse phenomenon.As Chinese invention patent (application No. is
201410025590.3) disclose a kind of method that normal pressure prepares aerosil, this method be through multiple exchange of solvent,
The modified classification under normal pressure in surface is dried to obtain aeroge.Li et al. people (Li Y, Tanna VA, Carter K R, et
al.Nanocellulose Aerogels Inspired by Frozen Tofu . ACS Sustainable Chem.
Eng. 2017,5,6387-6391.) inspiration prepared by food frozen bean curd utilizes Refrigeration Technique to improve cellulose gel
Mechanical stress, replaced using 2- propanol solvent and the gel that thaws successfully prepare complete cellulose finally by atmosphere pressure desiccation
Aeroge.
Summary of the invention
Goal of the invention: aiming at the problems existing in the prior art, the present invention provides a kind of compound airsetting of clay/sodium alginate
Glue flame resistant heat insulation material and preparation method thereof, the flame resistant heat insulation material that the present invention is prepared have extremely-low density, good machine
Tool performance, lower thermal conductivity and excellent flame retardant property have good application prospect in fields such as the flame resistant heat insulation materials of building.
Technical solution: the present invention provides a kind of clay/sodium alginate composite aerogel flame resistant heat insulation materials, by following matter
The group of amount ratio is grouped as: clay: calcium carbonate: sodium alginate: gluconolactone=100:1 ~ 5:5:1.75.
The present invention also provides a kind of clay/sodium alginate composite aerogel flame resistant heat insulation material preparation methods, including
Following steps: (1) clay with deionized water is configured to 2wt% clay slurry, appropriate calcium carbonate is added into clay slurry and beats
Slurry 10 ~ 30min of dispersion continuously adds 10 ~ 30min of appropriate 2wt% sodium alginate soln mashing dispersion and obtains mixed slurry；(2) will
(1) gained mixed slurry is slowly injected into gluconolactone with the rate of 3 ~ 5ml/min, is stood 6 ~ 12h of aging, is obtained hydrogel；
(3) hydrogel obtained by (2) is transferred to 3 ~ 4h of immersion in Isopropanol Water Solvent Mixtures, obtains alcogel；(4) solidifying to alcohol obtained by (3)
Glue carries out freezing processing, obtains that clay/sodium alginate is compound to congeal glue；(5) glue is congealed by clay/sodium alginate is compound obtained by (4)
It is put into isopropanol and thaws, and 6 ~ 12h is then replaced with isopropanol, obtain modified gel；(6) by modified gel obtained by (5)
It is put into constant pressure and dry case with 50 ° ~ 70 ° progress 10 ~ 12h of constant pressure and dry, obtains clay/sodium alginate anti-flaming thermal-insulation aeroge.
Preferably, in step (1), the additional amount of the calcium carbonate is 1 wt% ~ 5wt% of clay quality.
Preferably, in step (1), the additional amount of the sodium alginate is the 5wt% of clay quality.
Preferably, in step (2), the mass ratio of the sodium alginate and glucose lactones is 2:0.7.
Preferably, in step (3), the concentration of the Isopropanol Water Solvent Mixtures is 15% ~ 25%.
Preferably, in step (4), the temperature of the freezing processing is -80 DEG C ~ -196 DEG C, the processing time for 5min ~
15min。
Preferably, in step (5), the additional amount of the isopropanol is congeals compound more than the clay/sodium alginate
Colloid accumulates 10 ~ 15ml.
Preferably, the clay be through sufficiently dissociation processing fibrous type or sheet clay, preferably bentonite, it is recessed soil,
Sepiolite or reason saponite.
The utility model has the advantages that it is raw material that the present invention, which is widely present with nature and has the clay compared with high flame retardant, using seaweed
Sour sodium improves the mechanical performance of aeroge, and using Isopropanol Water Solvent Mixtures, gained hydrogel is chilled, isopropanol solvent
The aeroge that displacement and constant pressure and dry obtain has extremely-low density, and (its range is in 0.025g/cm3~0.058g/cm3), good machine
Tool performance, lower thermal conductivity (its range is at 0.020 ~ 0.032W/ (mk)) and excellent flame retardant property (it is unobvious to bear gas flame
Burning is greater than 300 seconds), have good application prospect in fields such as the flame resistant heat insulation materials of building.
The present invention has the advantages that
1. natural polymer sodium alginate constructs the frame structure of aeroge, clay all has good hydrophilic with sodium alginate
Property, compatibility is good, the good mechanical performance of the compound imparting aeroge of the two and ideal pore structure abundant；
2. natural minerals clay has good anti-flammability, material base is provided to prepare flame resistant heat insulation material.
3. constant pressure and dry technology provided by the invention prepares clay-based anti-flaming thermal-insulation aeroge, short preparation period (2 days) is molten
Agent consumption is few, and production cost is low, has good application prospect in the flame resistant heat insulation material field of building.
Detailed description of the invention
Fig. 1 is that EPS polystyrene block and the comparison of recessed soil/sodium alginate composite aerogel flame resistant heat insulation material flammability are real
Passport control examination of passports piece.
Fig. 2 is recessed soil/sodium alginate composite aerogel flame resistant heat insulation material burning front and back SEM micro-structure diagram.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawing.
Embodiment 1:
Present embodiments provide for a kind of recessed soil/sodium alginate composite aerogel flame resistant heat insulation materials, by the group of following mass ratio
It is grouped as: recessed soil: calcium carbonate: sodium alginate: gluconolactone=100:1:5:1.75.
Above-mentioned recessed soil/sodium alginate composite aerogel flame resistant heat insulation material is the preparation method is as follows: recessed soil is crushed to by (1)
200 mesh are added deionized water and are configured to 2wt% slurry, are beaten dispersion 30min, the non-recessed soil of centrifugal sedimentation sub-cloud with 10000rpm
Impurity.The precipitated calcium carbonate of the recessed soil property amount of 1wt% is added in the recessed soil paste material that deimpurity recessed soil will be gone to be reconfigured as 2wt%, with
After 10000rpm is sufficiently beaten dispersion 15min, 2wt% sodium alginate soln is added and continues to be beaten dispersion 30min with 10000rpm,
Obtain mixed slurry；Wherein, sodium alginate additional amount is the 5wt% of recessed soil property amount.(2) mixed slurry is delayed with the rate of 4ml/min
Slowly being injected into gelation 12h in gluconolactone obtains hydrogel；Wherein, sodium alginate and glucose lactones mass ratio are 2:0.7.
(3) hydrogel is placed in 20% Isopropanol Water Solvent Mixtures and shakes 3h on shaking table and obtain alcogel；Shaking table temperature controls
40 DEG C, speed 120rpm/min.(4) alcogel freezes 10min under -196 °C and obtains that recessed soil/sodium alginate is compound to congeal glue,
(5) the compound glue of congealing of recessed soil/sodium alginate is immersed in isopropanol the 6h that thaws, obtains modified gel.(6) modified gel is put into
With constant pressure and dry 10h at 60 DEG C in drying box, recessed soil/sodium alginate composite aerogel flame resistant heat insulation material is obtained；The heat-barrier material
Density be 0.035g/cm3, thermal conductivity 0.023Wm-1·K-1, receiving gas flame is unobvious, and burning is greater than 300 seconds.
Fig. 1 is that EPS polystyrene block and the comparison of recessed soil/sodium alginate composite aerogel flame resistant heat insulation material flammability are real
Passport control examination of passports piece.It is ignited using EPS polystyrene block moment, is burnt totally in 6 seconds as seen from Figure 1.And use compound airsetting
Glue cannot be lighted by open fire, partially carbonized phenomenon only occur, and no obvious flue gas generates.
Fig. 2 is recessed soil/sodium alginate composite aerogel flame resistant heat insulation material burning front and back SEM micro-structure diagram.It can from Fig. 2
To find out, before and after composite aerogel small fire experimental combustion, inter-particle voids become larger, but significant change does not occur in internal structure.
This illustrates that the interaction between recessed soil/sodium alginate system is formed by structure and can prevent turn of heat and combustible volatile
It moves.
Embodiment 2:
Present embodiments provide for a kind of sepiolite/sodium alginate composite aerogel flame resistant heat insulation materials, by following mass ratio
Group is grouped as: sepiolite: calcium carbonate: sodium alginate: gluconolactone=100:1:5:1.75.
Above-mentioned sepiolite/sodium alginate composite aerogel flame resistant heat insulation material the preparation method is as follows: (1) by sepiolite powder
200 mesh are broken to, deionized water is added and is configured to 2wt% slurry, dispersion 30min are beaten with 10000rpm, centrifugal sedimentation sub-cloud is non-
Sepiolite impurity.3wt% sepiolite quality is added in the sepiolite slurry that deimpurity sepiolite will be gone to be reconfigured as 2wt%
Precipitated calcium carbonate after being sufficiently beaten dispersion 10min with 10000rpm, is added the continuation of 2wt% sodium alginate soln and is beaten with 10000rpm
Slurry dispersion 30min, obtains mixed slurry；Wherein, sodium alginate additional amount is the 15wt% of sepiolite quality.(2) by mixed slurry with
The rate of 5ml/min is slowly injected into gelation 10h in gluconolactone and obtains hydrogel；Wherein, in sodium alginate and glucose
Rouge mass ratio is 2:0.7.(3) hydrogel is placed in 15% Isopropanol Water Solvent Mixtures and shakes 2h on shaking table and obtains alcohol and coagulated
Glue；The control of shaking table temperature is 40 DEG C, speed 120rpm/min.(4) alcogel freezes 15min under -80 °C, obtain sepiolite/
Sodium alginate is compound to congeal glue, and the compound glue of congealing of sepiolite/sodium alginate is immersed in isopropanol the 8h that thaws by (5), obtains modification
Gel.(6) modified gel is put into drying box with constant pressure and dry 11h at 65 DEG C, obtains sepiolite/sodium alginate composite aerogel
Flame resistant heat insulation material；The density of the heat-barrier material is 0.060g/cm3, thermal conductivity 0.029Wm-1·K-1, bear gas flame not
Obviously, burning is greater than 300 seconds.
Embodiment 3:
Present embodiments provide for a kind of recessed soil/sodium alginate composite aerogel flame resistant heat insulation materials, by the group of following mass ratio
It is grouped as: recessed soil: calcium carbonate: sodium alginate: gluconolactone=100:1:5:1.75.
Above-mentioned recessed soil/sodium alginate composite aerogel flame resistant heat insulation material is the preparation method is as follows: recessed soil is crushed to by (1)
200 mesh are added deionized water and are configured to 2wt% slurry, are beaten dispersion 25min, the non-recessed soil of centrifugal sedimentation sub-cloud with 10000rpm
Impurity.The precipitated calcium carbonate of the recessed soil property amount of 5wt% is added in the recessed soil paste material that deimpurity recessed soil will be gone to be reconfigured as 2wt%, with
After 10000rpm is sufficiently beaten dispersion 15min, 2wt% sodium alginate soln is added and continues to be beaten dispersion 30min with 10000rpm,
Obtain mixed slurry；Wherein, sodium alginate additional amount is the 3wt% of recessed soil property amount.(2) mixed slurry is delayed with the rate of 4ml/min
Slowly being injected into gelation 8h in gluconolactone obtains hydrogel；Wherein, sodium alginate and glucose lactones mass ratio are 2:0.7.
(3) hydrogel is placed in 15% Isopropanol Water Solvent Mixtures and shakes 3h on shaking table and obtain alcogel；Shaking table temperature controls
40 DEG C, speed 120rpm/min.(4) alcogel freezes 6min under -196 °C and obtains that recessed soil/sodium alginate is compound to congeal glue,
(5) the compound glue of congealing of recessed soil/sodium alginate is immersed in isopropanol the 8h that thaws, obtains modified gel.(6) modified gel is put into
With constant pressure and dry 12h at 70 DEG C in drying box, recessed soil/sodium alginate composite aerogel flame resistant heat insulation material is obtained；The heat-barrier material
Density be 0.025g/cm3, thermal conductivity 0.020Wm-1·K-1, receiving gas flame is unobvious, and burning is greater than 300 seconds.
The technical concepts and features of above embodiment only to illustrate the invention, its object is to allow be familiar with technique
People cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
The equivalent transformation or modification that Spirit Essence is done, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of clay/sodium alginate composite aerogel flame resistant heat insulation material, which is characterized in that be grouped by the group of following mass ratio
At: clay: calcium carbonate: sodium alginate: gluconolactone=100:1 ~ 5:5:1.75.
2. a kind of clay as described in claim 1/sodium alginate composite aerogel flame resistant heat insulation material preparation method, special
Sign is, comprising the following steps:
(1) clay is configured to 2wt% clay slurry with deionized water, appropriate calcium carbonate mashing dispersion is added into clay slurry
10 ~ 30min continuously adds 10 ~ 30min of appropriate 2wt% sodium alginate soln mashing dispersion and obtains mixed slurry；
(2) mixed slurry obtained by (1) is slowly injected into gluconolactone with the rate of 3 ~ 5ml/min, stands 6 ~ 12h of aging,
Obtain hydrogel；
(3) hydrogel obtained by (2) is transferred to 3 ~ 4h of immersion in Isopropanol Water Solvent Mixtures, obtains alcogel；
(4) freezing processing is carried out to alcogel obtained by (3), obtains that clay/sodium alginate is compound to congeal glue；
(5) by clay/sodium alginate obtained by (4) it is compound congeal glue and be put into isopropanol thaw, and then set with isopropanol
6 ~ 12h is changed, modified gel is obtained；
(6) modified gel obtained by (5) is put into constant pressure and dry case with 50 DEG C ~ 70 DEG C progress 10 ~ 12h of constant pressure and dry, obtain clay/
Sodium alginate composite aerogel anti-flaming thermal-insulation aeroge.
3. clay according to claim 1/sodium alginate composite aerogel flame resistant heat insulation material preparation method, feature
It is, in step (1), the additional amount of the calcium carbonate is 1 wt% ~ 5wt% of clay quality.
4. clay according to claim 1/sodium alginate composite aerogel flame resistant heat insulation material preparation method, feature
It is, in step (1), the additional amount of the sodium alginate is the 5wt% of clay quality.
5. clay according to claim 1/sodium alginate composite aerogel flame resistant heat insulation material preparation method, feature
It is, in step (2), the mass ratio of the sodium alginate and glucose lactones is 2:0.7.
6. clay according to claim 1/sodium alginate composite aerogel flame resistant heat insulation material preparation method, feature
It is, in step (3), the concentration of the Isopropanol Water Solvent Mixtures is 15% ~ 25%.
7. clay according to claim 1/sodium alginate composite aerogel flame resistant heat insulation material preparation method, feature
It is, in step (4), the temperature of the freezing processing is -80 DEG C ~ -196 DEG C, and the processing time is 5min ~ 15min.
8. clay according to claim 1/sodium alginate composite aerogel flame resistant heat insulation material preparation method, feature
Be, in step (5), the additional amount of the isopropanol be more than the compound jelly gel volume of the clay/sodium alginate 10 ~
15ml。
9. the preparation of clay according to any one of claim 1 to 8/sodium alginate composite aerogel flame resistant heat insulation material
Method, which is characterized in that the clay is fibrous type or sheet clay through sufficiently dissociation processing.
10. clay according to claim 9/sodium alginate composite aerogel flame resistant heat insulation material preparation method, special
Sign is that the clay is bentonite, recessed soil, sepiolite or reason saponite.
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| CN113150363A (en) * | 2021-02-06 | 2021-07-23 | 苏州大学 | Porous aerogel and preparation method thereof |
| CN113292761A (en) * | 2021-05-27 | 2021-08-24 | 淮阴工学院 | Preparation method of heat-insulating flame-retardant composite aerogel foam |
| CN114292446A (en) * | 2021-12-27 | 2022-04-08 | 重庆大学 | Glucomannan composite flame-retardant aerogel and preparation method thereof |
| CN115651274A (en) * | 2022-10-31 | 2023-01-31 | 淮阴工学院 | Preparation method of clay-based composite hydrogel for solar seawater desalination |
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| CN113292761A (en) * | 2021-05-27 | 2021-08-24 | 淮阴工学院 | Preparation method of heat-insulating flame-retardant composite aerogel foam |
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| CN115651274A (en) * | 2022-10-31 | 2023-01-31 | 淮阴工学院 | Preparation method of clay-based composite hydrogel for solar seawater desalination |
| CN115651274B (en) * | 2022-10-31 | 2024-03-26 | 淮阴工学院 | Preparation method of clay-based composite hydrogel for solar seawater desalination |
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